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By L. F. Willmott

The Bureau of Nines at Morgantown, W. Va., has been investigating, on a pilot plant scale, various methods of gasifying bituminous coal with oxygen and superheated steam to produce synthesis gas, as part of the broader program of finding new uses for coal. Differences in the pressure gasification methods used have depended on differences in the manner in which the pulverized coal is fed to the gasifier. One of the methods of feeding the coal that was investigated was the continuous, integrated coal-water slurry system. Goal and water were first mixed to produce a slurry; then the slurry was pumped through a heated coil. to evaporate the water fraction; the resulting steam was superheated, and some of it was separated so as to adjust the ratio of the residual steam to the coal fraction and make the resulting mixture suitable for partial combustion with oxygen in a pressure gasifier. Both before and during this reported3 developmental work it was necessary to make an extensive literature search into the technology of aqueous slurries in order to establish design criteria for the pilot plant and to correlate results of various phases of the work with that of other investigators, The pilot work coincided with the commercial development of a long-distance pipe- line for the transportation of coal as a coal-water slurry, and this fact tended to broaden the scope of the pilot plant work and the extent of the literature search. This bibliography is the compilation of the material that was collected.

Jan 1, 1963

By Robert E. Thurmond

With modern exploration techniques, it seems likely that an increasing number of the orebodies to be found in the future will be under alluvial fans or valley fill. As a result, a larger proportion of open pit mines will be confronted with the necessity for removal of substantial quantities of alluvial overburden; whereas in the past, for the most part, the open pit mine operator has dealt mainly with hard rock. If this proves to be the case, methods, equipment, and costs for alluvium stripping will become an increasingly important factor in open pit mine planning. Several operations are now faced with this situation, and various methods and equipment are used. At Pima Mining Company's operation the stripping ratio is in the range of 6/1 Well over half of the stripping volume is alluvium. The alluvium is removed almost entirely by carryalls hauling direct to a waste dump. Some removal has been accomplished by shovel and truck operation; more will be done by this means in the future. At American Smelting and Refining Company's neighboring .Mission Mine, nearly all alluvium removal is by large shovels and, trucks. U. S. Borax's Boron operation is accomplishing alluvium removal with carryalls but has been investigating other methods and equipment. The various operations in the Gas Hills Uranium District in Wyoming are stripping mainly with carryalls, although some small draglines are employed. The M. A. Hanna Company in the Mesabi Range employs large draglines and conveyor systems for removal of glacial fill. Nchanga Consolidated Copper Mines in Northern Rhodesia strips overburden with a large excavating wheel and conveyor system. There are no doubt other open pit operations with which the writer is not familiar, that are handling large quantities of alluvial overburden.

Jan 1, 1963

By L. J. E. Hofer

This Bureau of Mines study, part of a broad program of research in air pollution related to minerals, was conducted to determine the nature and extent of the poisoning of catalysts when used to remove certain air pollutants from exhaust gases. The poisoning examined in this investigation occurs when leaded gasoline is used as a fuel for automotive engines. This research was conducted in cooperation with the Public Health Service. The smog in the Los Angeles area is attributed to the effect of radiant energy on the mixture of hydrocarbons and nitrogen oxides found in the atmosphere there. A large portion of the hydrocarbons is believed to originate in the exhaust gases of automobiles. To prevent the escape of these hydrocarbons into the atmosphere catalytic mufflers have been proposed. In principle, these are simple and nonmechanical, consisting of a vessel charged with a catalyst capable of destroying the exhaust hydrocarbons by catalyzing their oxidation. However, these catalysts are severely affected by the particulate matter, mainly in the form of lead sulfate (PbS04), lead oxysulfate (PbS04.Pb0), and Lead chlorobromide (Pb(Cl,Br)2), contained in the exhaust gas. Deposition of lead on the catalyst as PbS04, PbS04, PbS0, and Pb(Cl,Br)2 restricts catalytic activity. As a result,after 20,000 miles of operation the temperature necessary to achieve 50-percent conversion of isopentane in a mixture of 0.2 percent isopentane, 2 percent carbon monoxide and 4 percent oxygen, and the balance nitrogen at 10,000 hourly space velocity has risen from 400° C. to 500° C. even with a catalyst taken from the exit portion of the catalyst bed. The rest of the catalyst was more severely affected. Therefore, it would appear that operation for 20,000 miles is near the limit for a catalyst.

Jan 1, 1963

By R. F. Abernethy

Recent investigations in the United States and in other countries have produced considerable information on the nature and occurrence of minor elements in coal. The possibility of recovering certain elements, particularly germanium and uranium, from coal ash and other coal products has received considerable attention. Some flue dusts are potential sources of germanium, and certain lignite deposits are potential sources of uranium, but industrial recovery of these elements has been limited to small quantities for technical and economic reasons. Considering the large amount of coal mined annually, a small percentage of a rare element may have industrial significance if an economical method of recovery can be developed. In 1944 information on the occurrence of rare elements in coal was reviewed in Bureau of Mines Technical Paper 669 (46).3 This report is a revision of that paper with the view of summarizing published information available for United States coals, and pertinent information concerning coals of other countries. Selected references from the original paper are retained. New references do not include all preliminary reports when more permanent literature describing complete projects is available. Consequently, the list of references should not be considered complete.

Jan 1, 1963

In Mount Isa voltage and frequency fluctuations caused. by haulage shaft operation gave considerable difficulties with the initial application of Atomic Absorption Spectro-photometry.The methods used to stabilise the various units ' have been described.- Some other difficulties and the means used to eliminate or reduce them together with a-modified burner design are also discussed.

Jan 1, 1963

By Kenneth H. Johnston

This report describes in detail three waterflooding projects and a pres-sure-maintenance project in Butler and Cowley Counties, Kans., that will be visited on the 1963 annual spring tour of the Kansas-Oklahoma Waterflood Association. Among the unique features of the projects are the flooding of five oil-producing horizons separately with injection water furnished by two water treating plants. Discussion of the individual projects includes information on their early history, the source and treatment of the injection fluids, oil production decline curves, and the results of water injection on oil production.

Jan 1, 1963

By James A. Wasson

This report summarizes the results and conclusions reached by various investigators who have attempted to determine the extent to which hydraulic fracturing will affect the secondary recovery of crude oil by waterflooding. It also discusses the most advantageous use of this well-stimulation method in waterflood projects. A thorough search of the literature was made, and pertinent information was abstracted from appropriate reports. A carefully designed and controlled program of formation fracturing is an effective aid in waterflooding because it increases water-injection and oil-production rates. Generally, fracturing has resulted in little or no reduction in ultimate oil recovery, but under certain circumstances recovery has been substantially increased.

Jan 1, 1963

By B. C. Allen, R. I. Jaffee, D. J. Maykuth

Wrought unalloyed iodide chromium, containing 39 to 95 ppm total interstitials, has a tensile transition temperature of —15°C. Re crystallizing at 1100°C causes the transition to rise to 90° to 390°C, depending on the purity, grain size, and cooling rate after annealing. At about the 100 ppm level, individual additions of carbon or nitrogen raise the transition of both wrought and recrystallized chromium by as much as 210°C, while oxygen has a lesser effect, and sulfur essentially no effect. High transitzon temperatures are exhibited by recrystallized and quenched chromium, and appear to be associated with the amount and distribution of inter-stitials. The latter cm be either in solid solution or in the form of precipitates within the grains or at the grain boundaries. Quench hardening in chromium is primarily caused by nitrogen. The hardness, re crystallization, and grain growth behavior of chromium with and without impurity additions were also investigated. BECAUSE of low density and good oxidation resistance, chromium-base alloys are potentially useful for elevated-temperature applications. The main deterrent to the use of chromium in structural applications is its lack of low-temperature ductility, especially in the recrystallized condition. Accumulated evidence has shown that the ductility of chromium is sensitive to purity. The objective of the current study was to determine the effect of common nonmetallic impurities on the tensile properties of high purity chromium. The separate effects of carbon, oxygen, nitrogen, and sulfur additions on the ductile-to-brittle transition were evaluated for wrought and recrystallized material after various cooling rates. EXPERIMENTAL WORK Unalloyed iodide chromium and seven impurity alloys containing individual carbon, oxygen, nitrogen, or sulfur additions were prepared in rod form. Nominal additions were 100 ppm C, N, and S, and 100 to 500 ppm O. The additions were about a factor of ten greater than the residual amounts in the unalloyed material. The seven alloys and two unalloyed compositions were consolidated into four-pound ingots by conventional consumable arc melting of pressed and welded electrodes under 0.5 atm of helium. Impurity additions were made to the electrode in the form of crushed master alloys. The impurity alloys were double melted to improve homogeneity. The ingots were broken down by extrusion at 1200°C in evacuated steel cans at a reduction ratio of 18 :1, using a molten borosilicate glass lubricant and a ram speed of 80 in. per min. The cans were removed by acid pickling, and the chromium core ground free of surface undulations. Cut lengths were sheathed in mild steel and swaged at 900°C until the core was about 1/4 in. in diam. Two additional 15-lb ingots of unalloyed chromium (ICr-3, ICr-4) were prepared by arc melting and broken down by 26:1 extrusion at 1250°C without a steel can. The billet was lubricated and protected from contamination by a coating of molten glass. The resulting extrusion was then sheath swaged as described previously. Representative chemical analyses of each of the materials, after removal of a 10-mil surface layer

Jan 1, 1963

By M. M. Wong

Electrolysis of titanium carbide and a material consisting of titanium, carbon, nitrogen, and oxygen as soluble anodes in Used electrolytes was investigated by the Bureau of Mines for the preparation of crude titanium metal. Tests made in all-chloride electrolytes showed only a low recovery of titanium as well as a substantial volatilization of titanium trichloride (TiC13) when present in the electrolyte. Electrolysis at 750° to 850° C in a mixture containing 85 percent NaC1-15 percent potassium floutitanate (K2TiF6) yielded as high as 91 percent recovery of titanium from titanium carbide and 62 percent recovery of titanium from the titanium-carbon-nitrogen-oxygen material. Problems associated with the preparation of crude metal by fused-salt electrolysis are discussed. The crude metals produced from both anode materials were electrorefined in a sodium chloride-titanium chloride (NaCl-TiC12) electrolyte, and ductile titanium metal was obtained.

Jan 1, 1963

By Martin H. Stanczyk

Acid leaching of selected copper sulfide minerals, impure copper sulfide flotation concentrates, and a cement copper precipitate at elevated temperatures and pressures was investigated. Copper extractions of 97 to 99 pct were obtained by leaching chalcopyrite and the flotation concentrates with water under oxidizing conditions at 200° C for 30 to 60 min. In tests with bornite, chalcocite,and cement copper, addition of sulfuric acid or pyrite to the autoclave was required to obtain similar copper extractions. The chemistry of leaching copper minerals was studied. It was determined that different copper sulfides altered to covellite as one step in their dissolution.

Jan 1, 1963

Australian rutile and zircon concentrates are refined raw materials and not manufactured products. The composition and properties of the grains are therefore fixed by nature. Specifications and assay certificates should take this into account by eliminating unnecessary provisions which only increase the time and cost of analysis.INTRODUCTIONThe raw material from which Australian rutile and zircon concentrates are isolated is beach sand on the coast of New South Wales and Southern Queensland. The principal current operations are in an area between Sydney and Brisbane.The sands consist principally of quartz particles, but they contain from 1 per cent to 50 per cent of a mixture of heavy minerals, including zircon, rutile, ilmenite, monazite, leucoxenic grains, chrome spinel, chromite, garnets, corundum, topaz, brown spinel, olivine, epidote, clinozoisite, tourmaline, magnetite, hematite, and cassiterite. The major components are zircon (25 to 60 per cent), rutile (25 to 50 per cent), and ilmenite (5 to 50 per cent).The so-called leucoxenic grains are not a definite mineral species but an alteration product of which the major components are titanium oxides and silica in varying proportions.Primary concentration is by gravity, using spirals or various forms of pinched sluice (Pullar, 1962), the resulting concentrates being redressed on wet tables. During these processes, some of the lighter heavy minerals including leucoxene and impure rutile, which tend to degrade the final rutile and zircon concentrates, are eliminated.The separation of heavy minerals from each other is...

Jan 1, 1963

By H. C. Carpenter

Lignite tar made by low-temperature Lurgi-Spülgas carbonization of North Dakota lignite was hydrocracked in single-pass, fixed-bed operation at 3,000 pounds per square inch over cobalt molybdate catalyst to produce gasoline, and at the same pressure, over zinc chromite catalyst to crack the high-boiling phenolic compounds to low-boiling phenolics. Hydrocracking the raw tar or the creosote-oil fraction from the tar over cobalt molybdate removed most of the oxygen, sulfur, and nitrogen in the forms of water, hydrogen sulfide, and ammonia, and produced gasoline yields from 31 to 59 volume-percent. The gasoline fractions contained from 0.1 to 7.7 volume-percent tar acids, but tar-base percentages were too low for reliable measurement; removal of these materials with dilute caustic and acid solutions also reduced the sulfur and nitrogen to 0.01 weight-percent or less.

Jan 1, 1963

By Robert Stefanko

Longwall mining appears very attractive from an engineering standpoint because of its simplicity. The use of one long, continuous face can simplify power distribution, ventilation, and supervision, and minimizes or prevents lost time associated with the tramming of equipment in room-and-pillar systems. Since the longwall system is more amenable to automation, it is inherently safer than room and pillar. Remote control of all face equipment from gate roads will obviate the exposure of men in the face area. Considering what has been said, it seems a paradox that more longwall installations are not found in the United States. However, with favorable mining conditions in relatively level seams of adequate height under shallow cover, it has been possible to develop highly productive, mechanized, room-and-pillar systems. Thus there has been no real incentive to employ longwall in the United States. In Europe, mining companies usually have very little choice between the two systems. Pitching seams of low height located at great depth dictate the use of longwall methods. With depletion of its readily accessible reserves, mining conditions will be similar to those now prevailing in Europe, and an increase in the use of longwall in the United States can be anticipated.

Jan 1, 1963

By D. R. Bomberger

An automatic microscope has been developed to .measure the size and populations of macerals and minerals in fine coal particles. Differentiations are made on the basis of reflectance. This study is concerned with the size distribution of pyrite inclusions. Most fine coal cleaning processes do not remove pyrite as completely as a straight density separation. Consideration of the pyrite size distribution is suggested as a more accurate method of predicting sulfur reduction by a cleaning process. Analyses of float-sink results and Deister Table operation in terms of pyrite particle sizes are made. Other potential applications of automatic microscopy are also discussed.

Jan 1, 1963

By Alla D. Mah

Energies of combustion of vanadium nitride (VN) and vanadium carbide (VC) were measured. Correcting to vanadium tetroxide (V204) as the final state, the heats of combustion were ?H298.15=-118,700±100 cal/mole of vanadium nitride and ?H298.15=-240,270±360 cal/mole of vanadium carbide. With vanadium pentoxide (V205) as the final state, the heats of combustion were ?H298.15= -133.440±100 cal/mole of vanadium nitride and ?H298.15=-255,020±360 cal/mole of vanadium carbide. Combining these results with vanadium oxide data, the heats of formation obtained were ?298.15=-51,880±200 cal/mole of vanadium nitride and ?H298.15=-24,350±400 cal/mole of vanadium carbide. Heats and free energies of formation of vanadium nitride and carbide were calculated to 2,000° K.

Jan 1, 1963

By S. Brunauer

The hydration of portland cement is treated as a chemical reaction and the changes in matter, in energy and the rate of change of the process are discussed, Portland cement is a mixture of four major and at least as many important minor constituents. In the hydration process, the four major compounds (trical-cium silicate, dicalcium silicate, tricalcium alumi-nate and tetracalcium aluminoferrite), plus gypsum and water form five or six new compounds. In spite o the great complexity of the reaction, considerable progress has been made in its understanding, primarily with the help of such research tools as X-ray diffraction and electron microscopy. The rate of the reaction can be followed by direct and indirect methods of measurements. The effects o composition, particle size (or specific surface), temperature and water-cement ratio on the rates of hydration are discussed. The hydration of portland cement is a chemical reaction accompanied by such highly important physical phenomena as heat evolution, setting and hardening. It is a vast and complex subject, on which hundreds of papers have been published. At the time of the writing of this paper, in October 1962, a two-volume book, which alone contains dozens of papers pertaining to cement hydration appeared in print.' The present paper deals with a few aspects of this vast subject, and the selection was not easy. The work reported here deals with some of the most recent investigations in the field. In any chemical reaction, the physical chemist is primarily interested in three things: changes in matter, changes in energy and the rate of change of the process or the speed of the reaction. This is true also of the chemical reaction between portland cement and water, and all three aspects of the reaction will be discussed. These three aspects are of vital interest to the engineer as well. Portland cement is not a cementing material — the hydration products, the new materials which form in the reaction, have the cementing action. The energy changes manifest themselves in a considerable evolution of heat, which may be useful or harmful. It is useful, for example, in winter concreting, but in very large concrete structures like dams, a large evolution of heat, which cannot be easily dissipated, may produce distress in the structure. Primarily for such a purpose was the Type IV or low heat portland cement developed. The speed of the chemical reaction is important because it determines the time of setting and hardening. The initial reaction must be slow enough to permit placing of the concrete before setting occurs. On the other hand, after the placing of concrete it is often highly desirable to obtain as rapid chemical reaction as possible. For this purpose the Type 111 or high early strength portland cement was developed. CHANGES IN MATTER Portland Cement: In a basic investigation, before one begins to study a reaction, one either knows the quantities and compositions of the starting materials, the reactants, or one determines them. This is obvious; the chemist expresses the changes in matter that occur in a reaction by a chemical equation, which has the quantities and compositions of the reactants on the left side of the equation and the quantities and compositions of the reaction products on the right side. The first question is then what to put on the left side of the equation in the reaction between portland cement and water? It is not very easy to answer this question. Portland cement is not a single chemical compound but a mixture of many compounds. Four of these are considered the major compounds, and at least four of the minor compounds also play important roles in the hydration reaction. In order to avoid complicating matters, the present discussion will be restricted primarily to the four major compounds, which constitute usually more than 90% of a portland cement. The relative amounts of these compounds vary from cement to cement. Actually not only the amounts but the compositions of these constituents also vary to some extent, but the variation in composition of the individual components will be neglected for simplicity.

Jan 1, 1963

By W. R. Hardwick

This Information Circular describes copper mining and concentrating methods, practices, and costs at the Silver Bell Unit of American Smelting and Refining Co., Pima County, Ariz. It is one of a series being prepared by the Bureau of Mines on mining methods, practices, and costs in various mining districts of the United States. The Silver Bell mining district, one of the older districts in Arizona, is in the western part of the Silver Bell Mountains in Pima County, about 40 miles west of Tucson and about 20 miles southwest of Red Rock, a station on the main line railroad of the Southern Pacific Co. The Oxide and the El Tiro open-pit mines of the American Smelting and Refining Co. are in the district (fig. 1. The principal ore deposits are in T. 12S., R.8E., Gila and Salt River base line, at an altitude of about 3,000 feet. The present town of Silver Bell, established in 1952, is reached by a paved highway, the Avra Valley road, that turns west from Highway 84 at Plata siding near Rillito and extends westward 25 miles to the townsite (fig. 2). The present town is about 5 miles southeast of the old town of Silver Bell that flourished from 1900 to 1930.

Jan 1, 1963

By A. A. Berk

Other Federal agencies have been coming to the Bureau of Mines for help with the purchase and utilization of fuel, largely coal, almost since the day the Bureau was created in 1910. The requests covered a wide range of fuel- economy problems and included boiler-water treatment after it became apparent that water-formed deposits on heating surfaces acted as insulators, decreasing heat transfer and impairing fuel efficiency. Dr. Ralph E. Hall, a Bureau of Mines physical chemist determined the 3 reactions that cause adhering scale to form in boilers (7)2 and went on to introduce scientific principles into water treatment for scale prevention (8). Widespread publicity of these achievements increased the requests for help from Federal steam-generating plants. Since no other Federal agency (even those which were more directly concerned with testing water) wanted to provide boiler-feedwater service, the Bureau decided to continue to give requested help to Federal agencies, Later, the Congress endorsed such agency cooperation as an economy measure,

Jan 1, 1963

By P. A. Bloom

Bureau of Mines research was conducted to develop effective separation methods that might be used in exploiting substantial tonnages of complex barite-fluorspar ores in Arizona. The exploitable reserves now may be increased as recent batch and continuous flotation tests demonstrated that a complex barite?-fluorspar ore from the Red Chief deposit, Yuma County, Ariz., could be selectively treated to concurrently produce (1) fluorspar and (2) a barite byproduct of marketable grade. The sample contained 24.8 percent CaF2 and 24.3 percent BaS04. Processing comprised production of a fluorspar product containing 97 percent CaF2 with an 82 percent recovery, using a sodium fluoride-lignin sulfonate-fatty acid reagent combination. Concurrent retreatment of the fluorspar tailing, using sodium cetyl sulfate as a collector, yielded a barite product of 94 percent BaS04 grade with a 71-percent recovery. The products met specifications for acid-grade fluorspar and drilling mud-type barite.

Jan 1, 1963

By A. R. Taylor

Low-temperature heat capacities of cesium chloride (7° - 300° K) and cesium iodide (13° - 300°K) were measured with an adiabatic calorimeter. The heat-capacity measurements were analyzed graphically to determine smooth values of heat capacity, entropy, enthalpy function, and free-energy function at 10° K intervals and at 273.15° and 298.15° K.

Jan 1, 1963